CN107777673A - A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof - Google Patents
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof Download PDFInfo
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- CN107777673A CN107777673A CN201711115797.XA CN201711115797A CN107777673A CN 107777673 A CN107777673 A CN 107777673A CN 201711115797 A CN201711115797 A CN 201711115797A CN 107777673 A CN107777673 A CN 107777673A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0765—Preparation by carboreductive nitridation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.Its technical scheme is：30 ~ 35wt% zirconia powder, 20 ~ 25wt% reducing agent, 28 ~ 31wt% magnesium chloride hexahydrate and 15 ~ 17wt% sodium chloride are mixed, obtain compound；Then under the conditions of nitrogen atmosphere, the compound is warming up to 700 ~ 1100 DEG C with 3 ~ 5 DEG C/min speed, 2 ~ 3h is incubated, natural cooling, obtains nitrogenizing product；The nitridation product is added again 1 ~ 2h is soaked in hydrochloric acid solution, with water washing is distilled 3 ~ 4 times, dried under the conditions of 110 DEG C, produce cube zirconium nitride powder based on low-temperature reduction.The concentration of the hydrochloric acid solution is 9 ~ 10wt%.The present invention has the characteristics of cost of material is low, safe, pollution-free, with short production cycle, technique is simple, synthesis temperature is low；Cube zirconium nitride powder purity based on low-temperature reduction prepared with this method is high and crystal development is good.
Description
Technical field
The invention belongs to zirconium nitride powder technology field.More particularly to a kind of cube zirconium nitride powder based on low-temperature reduction
And preparation method thereof.
Background technology
ZrN has many excellent physical and chemical properties, such as high-melting-point, high thermal stability, high rigidity, good wear-resisting
Property, good corrosion resistance and high-termal conductivity etc., therefore, it is commonly used as hard coat on cutting tool, actinium series fuel
Diffusion impervious layer and Josephson junction in inert base, integrated circuit.The synthesis of ZrN powder can pass through the direct of zirconium at present
Nitridation, the reacting, be double ion beam sputtered of zirconium chloride and ammonia, microwave plasma synthesis and SHS process.These sides
Though method has its advantage, very long reaction time or very high synthesis temperature are generally required.Thus ZrN powder is synthesized with other method
Paid close attention to by those skilled in the art at end：
E.Malikova et al.（E.Malikova, J.Pautova, A.Gromov, K.Monogarov, K.Larionov, U.
Teipel.On the mechanism of zirconium nitride formation by zirconium, zirconia
And yttria burning in air.Journal of Solid State Chemistry, 2015,230:199-208.）
Using Zr and ZrO2As primary raw material, Y2O3Burnt in atmosphere as additive, and combustion product is subjected to quenching and prepared
ZrN powder, this method are readily synthesized ZrN in atmosphere, but the cool time needs accurately to control, and the ZrN of synthesis purity is not high.
R.A.Shishkin et al.（R.A.Shishkin, E.S.Maiorova.Microwave vs Autoclave
Synthesis of Nanodisperse ZrN Powder. Glass and Ceramics, 2017,74:123-125.）Make
ZrN powder is synthesized with autoclave with microwave, this method is using zirconium chloride and sodium azide as primary raw material, isopropanol as molten
Agent, mixing 1 hour is carried out in a mixer.Mixture is placed in drying box and is evacuated to 10-3Pa, and be incubated at 50 DEG C
10h, add dimethylbenzene in the mixture afterwards, 24 hours are incubated at 250 DEG C by autoclave method, and carry out microwave heating 1
Hour synthesis zirconium nitride.This kind of method flow is more complicated, synthesis zirconium nitride cycle length, and used zirconium chloride is poisonous, is heated
Toxic chlorinated thing and the smog of compound containing zirconium are produced, sodium azide is poisonous drugs, is heated, contacts naked light or rubbed, shaken
It can be exploded when moving, hitting, safety issue be present.
Y.Li et al.（Y.Li, M.I.Jones.Synthesis of ZrN powders by aluminum-
reduction nitridation of ZrO2 powders with CaCO3Additive.Ceramics
International, 2017,43:3183-3189.）Zirconium nitride is prepared using thermit reduction, 1400 DEG C be incubated 6h and
By ZrO under 0.4MPa nitrogen pressure2-Al-CaCO3The higher zirconium nitride of reaction synthesis purity.This method need in higher temperatures and
Reacted under certain pressure, soaking time length, severe reaction conditions, be unfavorable for industrialized production.
B.Fu et al.（B.Fu, L.Gao.Synthesis of Nanocrystalline Zirconium Nitride
Powders by Reduction-Nitridation of Zirconium Oxide.Journal of the American
Ceramic Society, 2004,87:696-698.）Reduction nitridation nanometer ZrO in using magnesium as reducing agent, ammonia2Powder,
1000 DEG C of insulation 6h successfully synthesize 30 ~ 100nm pure phase cube ZrN powders., as nitrogen source, peace be present using ammonia in this method
Full sex chromosome mosaicism, and nitridation time is grown.
Though zirconium nitride prepared by these methods obtains significant progress, the reaction of high reaction temperature, length is needed mostly
, there is safety issue in time and complicated operating process or yield is low etc..
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide that a kind of cost is low, synthesis temperature is low, the production cycle
It is short, technique is simple, the pollution-free and safe cube zirconium nitride raw powder's production technology based on low-temperature reduction, use this method
Cube zirconium nitride powder purity based on low-temperature reduction prepared is high and crystal development is good.
To achieve the above object, the technical solution adopted in the present invention is：By 30 ~ 35wt% zirconia powder, 20 ~ 25wt%
Reducing agent, 28 ~ 31wt% magnesium chloride hexahydrate and 15 ~ 17wt% sodium chloride mixing, obtain compound；Then in nitrogen atmosphere
Under the conditions of, the compound is warming up to 700 ~ 1100 DEG C with 3 ~ 5 DEG C/min speed, 2 ~ 3h is incubated, natural cooling, obtains nitrogen
Change product；The nitridation product is added again 1 ~ 2h is soaked in hydrochloric acid solution, with distillation water washing 3 ~ 4 times, under the conditions of 110 DEG C
Drying, produces cube zirconium nitride powder based on low-temperature reduction.
The concentration of the hydrochloric acid solution is 9 ~ 10wt%.
Purity >=99.0wt% of the zirconia powder；Granularity≤0.1mm of the zirconia powder.
The reducing agent be magnesium powder, aluminium powder and activated carbon in one kind, purity >=99.5wt%；The reducing agent granularity≤
0.1mm。
Purity >=99.5wt% of the magnesium chloride hexahydrate；Granularity≤0.1mm of magnesium chloride hexahydrate.
Purity >=99.5wt% of the sodium chloride；Granularity≤0.1mm of sodium chloride.
Due to there is following good effect compared with prior art using above-mentioned technical proposal, the present invention：
The present invention is using zirconium oxide and reducing agent as primary raw material, and using magnesium chloride hexahydrate and sodium chloride as fused salt, cost is cheap；In nitrogen
2 ~ 3h is incubated under the conditions of gas atmosphere and 700~1100 DEG C, then the nitridation product of generation is washed away into impurity with hydrochloric acid and distilled water, is made
Cube zirconium nitride powder based on low-temperature reduction is obtained, this method is not only safe and pollution-free, and synthesis temperature is low, production week
Phase is short and technique is simple.
The present invention, as fused salt, is produced liquid phase environment using fused salt, promoted at high temperature using magnesium chloride hexahydrate and sodium chloride
Enter the mobility of reactant and improve reaction rate, and then reduce synthesis temperature and shorten the reaction time.Because fused salt is through generation
Particle between, can prevent to reunite between particle, or weakly agglomerated body generation, and generate powder structure it is uniform.In addition,
In course of reaction and subsequent cleaning process, be advantageous to the removing of impurity, the prepared cube nitrogen based on low-temperature reduction
It is high to change zirconium powder thing phase purity, grain diameter is 50 ~ 100nm, and crystal development is good.
Therefore, the present invention is with cost of material is low, safe, pollution-free, with short production cycle, technique is simple, synthesis temperature
Spend the characteristics of low.Cube zirconium nitride powder purity based on low-temperature reduction prepared with this method is high and crystal development is good.
Brief description of the drawings
Fig. 1 is a kind of XRD of cube zirconium nitride powder based on low-temperature reduction prepared by the present invention；
Fig. 2 is the SEM figures of cube zirconium nitride powder based on low-temperature reduction shown in Fig. 1.
Embodiment
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
In present embodiment：
The concentration of the hydrochloric acid solution is 9 ~ 10wt%.
Purity >=99.0wt% of the zirconia powder；Granularity≤0.1mm of zirconia powder.
Purity >=99.5wt% of the magnesium chloride hexahydrate；Granularity≤0.1mm of magnesium chloride hexahydrate.
Purity >=99.5wt% of the sodium chloride；Granularity≤0.1mm of sodium chloride.
Purity >=99.5wt% of the reducing agent；Granularity≤0.1mm of reducing agent.
Repeated no more in embodiment.
Embodiment 1
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.Preparation method is described in the present embodiment：
By 30 ~ 33wt% zirconia powder, 22 ~ 25wt% reducing agent, 29 ~ 30wt% magnesium chloride hexahydrate and 15.5 ~ 16.5wt%
Sodium chloride mixing, obtain compound；Then under the conditions of nitrogen atmosphere, with 3 ~ 4 DEG C/min speed by the compound liter
Temperature is incubated 2 ~ 3h, natural cooling, obtains nitrogenizing product to 700 ~ 900 DEG C；The nitridation product is added in hydrochloric acid solution again and soaked
1 ~ 2h is steeped, with water washing is distilled 3 ~ 4 times, is dried under the conditions of 110 DEG C, produces cube zirconium nitride powder based on low-temperature reduction.
The reducing agent is magnesium powder.
Embodiment 2
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.The present embodiment is aluminium powder except the reducing agent
Outside, remaining is the same as embodiment 1.
Embodiment 3
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.The present embodiment is activated carbon except the reducing agent
Outside, remaining is the same as embodiment 1.
Embodiment 4
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.Preparation method is described in the present embodiment：
By 31 ~ 34wt% zirconia powder, 21 ~ 24wt% reducing agent, 30 ~ 31wt% magnesium chloride hexahydrate and 15 ~ 16wt% chlorine
Change sodium mixing, obtain compound；Then under the conditions of nitrogen atmosphere, with 3.5 ~ 4.5 DEG C/min speed by the compound liter
Temperature is incubated 2 ~ 3h, natural cooling, obtains nitrogenizing product to 800 ~ 1000 DEG C；The nitridation product is added in hydrochloric acid solution again
1 ~ 2h is soaked, with water washing is distilled 3 ~ 4 times, is dried under the conditions of 110 DEG C, produces cube nitridation zirconium powder based on low-temperature reduction
Body.
The reducing agent is magnesium powder.
Embodiment 5
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.The present embodiment is aluminium powder except the reducing agent
Outside, remaining is the same as embodiment 4.
Embodiment 6
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.The present embodiment is activated carbon except the reducing agent
Outside, remaining is the same as embodiment 4.
Embodiment 7
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.Preparation method is described in the present embodiment：
By 32 ~ 35wt% zirconia powder, 20 ~ 23wt% reducing agent, 28 ~ 29wt% magnesium chloride hexahydrate and 16 ~ 17wt% chlorine
Change sodium mixing, obtain compound；Then under the conditions of nitrogen atmosphere, the compound is warming up to 4 ~ 5 DEG C/min speed
900 ~ 1100 DEG C, 2 ~ 3h is incubated, natural cooling, obtains nitrogenizing product；The nitridation product is added in hydrochloric acid solution again and soaks 1
~ 2h, with water washing is distilled 3 ~ 4 times, dried under the conditions of 110 DEG C, produce cube zirconium nitride powder based on low-temperature reduction.
The reducing agent is magnesium powder.
Embodiment 8
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.The present embodiment is aluminium powder except the reducing agent
Outside, remaining is the same as embodiment 7.
Embodiment 9
A kind of cube zirconium nitride powder based on low-temperature reduction and preparation method thereof.The present embodiment is activated carbon except the reducing agent
Outside, remaining is the same as embodiment 7.
Present embodiment has following good effect compared with prior art：
Present embodiment is using zirconium oxide and reducing agent as primary raw material, using magnesium chloride hexahydrate and sodium chloride as fused salt, cost
It is cheap；2 ~ 3h is incubated under the conditions of nitrogen atmosphere and 700~1100 DEG C, then the nitridation product hydrochloric acid of generation and distillation are washed
Decontamination, cube zirconium nitride powder based on low-temperature reduction is made, this method is not only safe and pollution-free, and synthesis temperature
Low, with short production cycle and technique is simple.
Present embodiment, as fused salt, liquid phase is produced using fused salt at high temperature using magnesium chloride hexahydrate and sodium chloride
Environment, promote the mobility of reactant and improve reaction rate, and then reduce synthesis temperature and shorten the reaction time.Because fused salt passes through
Between wearing the particle of generation, it can prevent to reunite between particle, or the generation of weakly agglomerated body, and the powder structure generated is equal
It is even.In addition, in course of reaction and subsequent cleaning process, be advantageous to the removing of impurity, it is prepared based on low-temperature reduction
Cube zirconium nitride powder thing phase purity it is high, grain diameter is 50 ~ 100nm, and crystal development is good.
Cube zirconium nitride powder based on low-temperature reduction prepared by present embodiment as depicted in figs. 1 and 2, Fig. 1
A kind of XRD of cube zirconium nitride powder based on low-temperature reduction is prepared for embodiment 1；Fig. 2 be Fig. 1 shown in based on low temperature also
The SEM figures of former cube zirconium nitride powder.It can be seen that from Fig. 1 and Fig. 2：Cube nitridation zirconium powder based on low-temperature reduction prepared
Body thing phase purity is high, and grain diameter is 50 ~ 100nm, and crystal development is good.
Therefore, present embodiment has that cost of material is low, safe, pollution-free, with short production cycle, technique is simple
Singly, the characteristics of synthesis temperature is low.Cube zirconium nitride powder purity based on low-temperature reduction prepared with this method is high and crystal is sent out
Cultivate.
Claims (6)
- A kind of 1. cube zirconium nitride raw powder's production technology based on low-temperature reduction, it is characterised in that：By 30 ~ 35wt% oxidation The sodium chloride mixing of zirconium powder, 20 ~ 25wt% reducing agent, 28 ~ 31wt% magnesium chloride hexahydrate and 15 ~ 17wt%, obtains compound； Then under the conditions of nitrogen atmosphere, the compound is warming up to 700 ~ 1100 DEG C with 3 ~ 5 DEG C/min speed, is incubated 2 ~ 3h, Natural cooling, obtain nitrogenizing product；The nitridation product is added again 1 ~ 2h is soaked in hydrochloric acid solution, with distillation water washing 3 ~ 4 It is secondary, dried under the conditions of 110 DEG C, produce cube zirconium nitride powder based on low-temperature reduction；The concentration of the hydrochloric acid solution is 9 ~ 10wt%.
- 2. cube zirconium nitride raw powder's production technology based on low-temperature reduction according to claim 1, it is characterised in that described Purity >=99.0wt% of zirconia powder；Granularity≤0.1mm of the zirconia powder.
- 3. cube zirconium nitride raw powder's production technology based on low-temperature reduction according to claim 1, it is characterised in that described Reducing agent be magnesium powder, aluminium powder and activated carbon in one kind, purity >=99.5wt%；Reducing agent granularity≤the 0.1mm.
- 4. cube zirconium nitride raw powder's production technology based on low-temperature reduction according to claim 1, it is characterised in that described Purity >=99.5wt% of magnesium chloride hexahydrate；Granularity≤0.1mm of magnesium chloride hexahydrate.
- 5. cube zirconium nitride raw powder's production technology based on low-temperature reduction according to claim 1, it is characterised in that described Purity >=99.5wt% of sodium chloride；Granularity≤0.1mm of sodium chloride.
- A kind of 6. cube zirconium nitride powder based on low-temperature reduction, it is characterised in that cube zirconium nitride based on low-temperature reduction Powder is prepared by cube zirconium nitride raw powder's production technology based on low-temperature reduction according to any one of right 1 ~ 5 Cube zirconium nitride powder based on low-temperature reduction.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483414A (en) * | 2018-04-16 | 2018-09-04 | 武汉科技大学 | One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof |
| CN108545707A (en) * | 2018-04-23 | 2018-09-18 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on liquid phase carbothermy |
| CN108569680A (en) * | 2018-04-23 | 2018-09-25 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on low temperature nitride |
| WO2022092274A1 (en) * | 2020-11-02 | 2022-05-05 | 三菱マテリアル株式会社 | Zirconium-containing nitride powder and ultraviolet ray-curable black organic composition |
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| CN108483414A (en) * | 2018-04-16 | 2018-09-04 | 武汉科技大学 | One kind is based on molten-salt growth method low temperature synthesis rhombohedral boron nitride powder and preparation method thereof |
| CN108545707A (en) * | 2018-04-23 | 2018-09-18 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on liquid phase carbothermy |
| CN108569680A (en) * | 2018-04-23 | 2018-09-25 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on low temperature nitride |
| WO2022092274A1 (en) * | 2020-11-02 | 2022-05-05 | 三菱マテリアル株式会社 | Zirconium-containing nitride powder and ultraviolet ray-curable black organic composition |
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